WO2016169408A1 - Composition de fibres de verre de haute performance, fibre de verre de cette dernière, et matériau composite - Google Patents

Composition de fibres de verre de haute performance, fibre de verre de cette dernière, et matériau composite Download PDF

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Publication number
WO2016169408A1
WO2016169408A1 PCT/CN2016/078518 CN2016078518W WO2016169408A1 WO 2016169408 A1 WO2016169408 A1 WO 2016169408A1 CN 2016078518 W CN2016078518 W CN 2016078518W WO 2016169408 A1 WO2016169408 A1 WO 2016169408A1
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WIPO (PCT)
Prior art keywords
glass
glass fiber
mgo
cao
ratio
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PCT/CN2016/078518
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English (en)
Chinese (zh)
Inventor
章林
曹国荣
邢文忠
顾桂江
洪秀成
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巨石集团有限公司
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Application filed by 巨石集团有限公司 filed Critical 巨石集团有限公司
Priority to BR112017022438-0A priority Critical patent/BR112017022438B1/pt
Priority to US15/565,412 priority patent/US10399889B2/en
Priority to ES16782556T priority patent/ES2828726T3/es
Priority to DK16782556.1T priority patent/DK3287425T3/da
Priority to EP16782556.1A priority patent/EP3287425B1/fr
Publication of WO2016169408A1 publication Critical patent/WO2016169408A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C13/00—Fibre or filament compositions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2213/00—Glass fibres or filaments

Definitions

  • the present invention relates to a high performance glass fiber composition, and more particularly to a high performance glass fiber composition capable of reinforcing a substrate as an advanced composite material, and glass fibers and composite materials thereof.
  • Glass fiber is an inorganic fiber material, and it can be used to reinforce a resin to obtain a composite material with excellent properties.
  • high-performance glass fiber was originally used in the defense, military and other fields of defense, military and other fields. With the advancement of technology and economic development, high-performance glass fiber has been widely used in civil and industrial fields such as motors, wind blades, pressure vessels, offshore oil pipelines, sports equipment, and the automotive industry.
  • the main components of Gaoqiang 2# glass fiber also include SiO 2 , Al 2 O 3 , MgO, and also introduce some parts of Li 2 O, B 2 O 3 , CeO 2 and Fe 2 O 3 , which also have high strength and Modulus, and its molding temperature is only about 1245 ° C, the liquidus temperature is 1320 ° C, the temperature of both is much lower than S glass fiber, but its molding temperature is lower than the liquidus temperature, but it is not good for glass fiber. Drawing, the drawing temperature must be increased, and a special form of the leaking nozzle is used to prevent the glass from devitrifying during the drawing process, which causes difficulty in temperature control and is difficult to achieve large-scale industrial production.
  • the present invention is directed to solving the problems described above. It is an object of the present invention to provide a high performance glass fiber composition which not only significantly improves the mechanical properties of the glass, but also makes it higher than conventional R glass; and can also greatly reduce the viscosity and crystallization risk of the glass. A lower liquidus temperature, wire drawing temperature and number of bubbles are obtained, making it significantly lower than conventional R glass, making the glass fiber composition more suitable for large scale kiln production.
  • a glass fiber composition comprising the following components, the content of each component being expressed by weight percentage as follows:
  • the glass fiber composition further comprises SrO, and the weight percentage of SrO is 0-2%.
  • the content of SrO is represented by 0.2 to 1.5% by weight.
  • the molar ratio ratio C1 Li 2 O/Al 2 O 3 ranges from 0.105 to 0.22
  • the weight percentage ratio C3 ( The range of MgO+SrO)/CaO is from 0.58 to 0.9.
  • a glass fiber made of the above glass fiber composition.
  • a composite material comprising the glass fibers described above.
  • the glass fiber composition of the present invention by introducing a higher content of Li 2 O, the content of the percentage by weight of CaO and MgO, the molar ratio of MgO/(CaO+MgO) and Li 2 O/Al 2 O 3 are appropriately arranged.
  • the use of Li 2 O and Al 2 O 3 , Li 2 O and MgO, CaO and MgO combination effect can not only significantly improve the mechanical properties of the glass, making it higher than the conventional R glass; but also can greatly reduce the viscosity of the glass and The crystallization risk, obtaining a lower liquidus temperature, wire drawing temperature and number of bubbles, makes it significantly lower than conventional R glass, making the glass fiber composition more suitable for large-scale kiln production.
  • the present invention can selectively introduce an appropriate amount of SrO, and further enhance the above advantageous technical effects by utilizing the ternary mixed alkaline earth effect of CaO, MgO, and SrO.
  • the glass fiber composition according to the present invention contains the following components, and the content of each component is expressed by weight percentage as follows:
  • the functions and contents of the components in the glass fiber composition are as follows:
  • SiO 2 is the main oxide forming the glass skeleton and functions to stabilize the components.
  • the content of SiO 2 is limited to 58.5-62.5%, and if the content is too low, the mechanical properties of the glass are affected; if the content is too high, the viscosity of the glass is too high to cause melting, Clarify the difficulties.
  • the content of SiO 2 may be limited to 59-62%.
  • Al 2 O 3 is a glass network intermediate oxide, which has two coordination states of tetracoordinate (tetrahedron) and hexacoordinate (octahedron), and is a conditional glass former.
  • tetracoordinate tetrahedron
  • octahedron hexacoordinate
  • AlO 6 aluminum octahedron
  • Al 2 O 3 can be promoted into the glass network structure in the form of aluminum oxide tetrahedron [AlO 4 ], and is affected by the accumulation of large field strong metal ions, and the structure of Al 2 O 3 to the network structure.
  • the reinforcing effect is more remarkable, which not only improves the mechanical properties of the glass, but also reduces the risk of crystallization of the glass.
  • the high content of Li 2 O just meets the above conditions. The inventors have found that Li 2 O not only provides considerable free oxygen, but also has a strong ion field strength, which facilitates the formation of tetrahedral coordination of more aluminum ions, thereby enhancing the network structure of the glass. Therefore, it is important to select the appropriate content and ratio of Al 2 O 3 and Li 2 O.
  • the range of 2 O/Al 2 O 3 is 0.105-0.22.
  • CaO is a glass network exosome oxide with only six coordination states. It can adjust the viscosity of the glass, control the crystallization of the glass, increase the strength of the glass, and shorten the glass frit and increase the molding speed of the glass fiber. MgO is also a glass network exosome oxide. There are two coordination states (tetrahedral) and six coordination (octahedron), most of which are located in octahedrons. MgO can also adjust the viscosity of the glass, control the crystallization of the glass, and is more conducive to increasing the modulus of the glass. When replacing part of CaO with MgO, the glass frit becomes gentle.
  • the crystal phase contained in the high-performance glass mainly composed of MgO-CaO-Al 2 O 3 -SiO 2 system mainly includes diopside (CaMgSi 2 O 6 ) and anorthite (CaAl 2 Si 2 O 8 ). .
  • diopside CaMgSi 2 O 6
  • anorthite CaAl 2 Si 2 O 8
  • the molecular formula Ca 2+ /Mg 2+ molar ratio of diopside is 1.
  • Ca 2+ and Mg 2+ it is necessary to have sufficient Ca 2+ and Mg 2+ at the same time.
  • anorthite is also An environment rich in Ca 2+ is needed to grow quickly.
  • the significant decrease in the degree of crystallization of the crystal phase is manifested by the significant decrease in the intensity of the X-ray diffraction peak, and the grain morphology of the diopside in the SEM scan of the crystal phase changes from column to rod to slender needle. It becomes smaller and the integrity is reduced.
  • the content of CaO is limited to a range of from 10.5 to 14.5%
  • the content of MgO is in the range of from 8 to 10%
  • the content of CaO ranges from 11.8 to 14.5%
  • the range of C2 MgO / (CaO + MgO) is from 0.44 to 0.53.
  • Both K 2 O and Na 2 O reduce the viscosity of the glass and are good fluxing agents.
  • replacing Na 2 O with K 2 O can reduce the crystallization tendency of the glass and improve the fiber forming property; and can also lower the surface tension of the glass liquid and improve the glass melting performance. Therefore, in the glass fiber composition of the present invention, the content of Na 2 O is limited to 0.05-1%, and the content of K 2 O is in the range of 0.05 to 1%, and a good effect can be obtained.
  • Fe 2 O 3 is advantageous for the melting of glass and also for improving the crystallization properties of glass.
  • the amount of introduction is not preferable. Therefore, in the glass fiber composition of the present invention, the content of Fe 2 O 3 is limited to a range of 0.05 to 1%.
  • TiO 2 not only reduces the viscosity of the glass at high temperatures, but also has a certain fluxing effect. Therefore, TiO 2 is added to the glass fiber composition of the present invention, and the content of TiO 2 is limited to a range of from 0.15 to 1.5%.
  • the present invention can also selectively introduce an appropriate amount of SrO, and further enhance the above advantageous technical effects by utilizing the ternary mixed alkaline earth effect of CaO, MgO, and SrO.
  • the inventors have found through a large number of studies that the technical effects of the mixed alkaline earth effect of CaO, MgO and SrO are significantly improved compared with the mixed alkaline earth effect of CaO and MgO under the premise of reasonable ratio. This is because more alkaline earth ions of different radii are involved in the substitution, and the structure is more likely to form close packing, thereby making the crystallization property and mechanical properties of the glass more excellent.
  • the crystallization process of glass is actually the process of nucleation and continuous growth, which is the process of reorganization and reorganization of various atoms in glass.
  • the ternary alkaline earth system designed in the invention is more likely to realize the close packing of the glass structure, and at the same time, due to the large ionic radius of Sr 2+ , it is not only difficult to move by itself, but also can effectively block Mg 2+ and Ca 2+ ions under the same conditions.
  • the mobile recombination achieves the purpose of suppressing the tendency of crystallization and reducing the rate of crystallization. Therefore, the glass fiber composition of the present invention can obtain more excellent glass crystallization properties.
  • the ternary mixed alkaline earth effect of CaO, MgO and SrO is comprehensively considered and the appropriate SrO content is selected to achieve lower liquidus temperature and crystallization degree, and higher mechanical properties.
  • the present invention defines the content of SrO in the range of 0 to 2%.
  • the content of SrO ranges from 0.2 to 1.5%
  • the glass fiber composition according to the present invention contains the following components, and the content of each component is expressed by weight percentage as follows:
  • the glass fiber composition according to the present invention contains the following components, and the content of each component is expressed by weight percentage as follows:
  • the glass fiber composition according to the present invention contains the following components, and the content of each component is expressed by weight percentage as follows:
  • the molar ratio ratio C1 Li 2 O/Al 2 O 3 ranges from 0.105 to 0.22
  • the weight percentage ratio C3 ( The range of MgO+SrO)/CaO is from 0.58 to 0.9.
  • each component in the glass fiber composition according to the present invention can not only significantly improve the mechanical properties of the glass, but also make it higher than the conventional R glass; and can also greatly reduce the viscosity and crystallization risk of the glass, and obtain a lower
  • the liquidus temperature and the wire drawing temperature make it significantly lower than conventional R glass, making the glass fiber composition more suitable for large-scale kiln production.
  • the specific content values of SiO 2 , Al 2 O 3 , CaO, MgO, Li 2 O, Na 2 O, K 2 O, Fe 2 O 3 , TiO 2 and SrO in the glass fiber composition of the present invention are selected as examples. Compare with the performance parameters of traditional E glass and traditional R glass. In performance comparison, six performance parameters are selected:
  • the molding temperature corresponds to the temperature at which the glass melt has a viscosity of 10 3 poise.
  • the liquidus temperature corresponds to the temperature at which the crystal nucleus begins to form when the glass melt is cooled, that is, the upper limit temperature of the glass crystallization.
  • Young's modulus which is the elastic modulus along the longitudinal direction, characterizing the ability of the glass to resist elastic deformation, tested according to ASTM 2343.
  • the number of bubbles wherein the approximate method of measuring the number of bubbles is: using a special mold to press each sample batch into a sample of the same shape, placed in a sample platform of a high temperature microscope, and then programmed to a set space temperature. At 1500 ° C, the glass samples were cooled to room temperature with the furnace; then, the number of bubbles of each glass sample was observed from a microscopic angle by a polarizing microscope. Among them, the number of bubbles is based on the imaging range of the microscope.
  • each component can be obtained from a suitable raw material, and various raw materials are mixed in proportion to achieve the final expected weight percentage of each component, and the mixed batch material is melted and clarified, and then the glass liquid
  • the glass fiber is formed by the leaking nozzle on the drain plate being pulled out, and the glass fiber is drawn around the rotating head of the wire drawing machine to form a raw silk cake or a yarn group.
  • these glass fibers can be further processed in a conventional manner to meet the expected requirements.
  • the above-described embodiments of the glass fiber composition of the present invention and other examples are further given below by way of a list. Comparison with the performance parameters of conventional E glass, conventional R glass and modified R glass. Wherein, the content of the glass fiber composition is expressed by weight percentage. It should be noted that the total content of the components of the examples is slightly less than 100%, and it can be understood that the residual amount is a trace impurity or a small component which cannot be analyzed.
  • the glass fiber composition of the present invention has the following advantages as compared with the conventional R glass and the modified R glass: (1) having a much lower liquidus temperature, which is advantageous for reducing the glass analysis. Crystal risk, improve fiber The drawing efficiency of the dimension; (2) the significantly improved mechanical properties; (3) the much lower number of bubbles, which indicates that the quality of the glass liquid of the present invention is greatly improved.
  • the glass fiber composition of the present invention has made a breakthrough in the improvement of the crystallization risk and the improvement of the mechanical properties of the R-grade glass, and the number of bubbles under the same conditions is significantly reduced, and the overall technical scheme is improved compared with the conventional R glass.
  • R glass fiber is easier to achieve large-scale industrial production.
  • the invention adopts a higher content of Li 2 O, reasonably configures the weight percentage content of CaO and MgO, the molar ratio ratio range of MgO/(CaO+MgO) and Li 2 O/Al 2 O 3 , and utilizes Li 2 O and Al.
  • the combination effect of 2 O 3 , Li 2 O and MgO, CaO and MgO can not only significantly improve the mechanical properties of the glass, but also make it higher than the traditional R glass; it can also greatly reduce the viscosity and crystallization risk of the glass, and obtain lower The liquidus temperature, wire drawing temperature and number of bubbles make it significantly lower than conventional R glass. Therefore, the glass fiber composition of the present invention is more suitable for large scale kiln production.
  • Glass fibers having the above-described excellent properties can be produced from the glass fiber composition according to the present invention.
  • the glass fiber composition according to the present invention can be combined with one or more organic and/or inorganic materials to produce a composite material having excellent properties, for example, a glass fiber reinforced substrate.
  • the composition of the invention can not only significantly improve the mechanical properties of the glass, but also make it higher than the conventional R glass; and can also greatly reduce the viscosity and crystallization risk of the glass, and obtain lower liquidus temperature, wire drawing temperature and number of bubbles. It is significantly lower than traditional R glass and is more suitable for large-scale kiln production.
  • the glass fiber composition of the invention has made a breakthrough in tensile strength, crystallization performance and Young's modulus, and the mechanical properties of the glass are greatly improved and crystallized under the same conditions. The risk is significantly reduced and the overall technical solution is particularly suitable for high performance fiberglass for large scale kiln production.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

La présente invention concerne une composition de fibres de verre de haute performance, la fibre de verre de cette dernière, et un matériau composite. La composition de fibres de verre comprend les composants suivants en pourcentage en poids : de 58,5 % à 62,5 % de SiO2, de 14,5 % à 17 % de Al2O3, de 10,5 % à 14,5 % de CaO, de 8 % à 10 % de MgO, Li2O ayant un pourcentage en poids supérieur à 0,5 % et inférieur ou égale à 1 %, de 0,05 % à 1 % de Na2O, de 0,05 % à 1 % de K2O, de 0,05 % à 1 % de Fe2O3, et de 0,15 % à 1,5 % de TiO2, où le rapport des pourcentages en mole C1=Li2O/Al2O3 s'étend de 0,105 à 0,22, et le rapport des pourcentages en mole C2=MgO/(CaO+MgO) s'étend de 0,435 à 0,55. La composition peut améliorer la performance mécanique du verre, réduire la viscosité du verre, les risques de cristallisation et le nombre de bulles, et convient mieux à la production à grande échelle de fours à cuve.
PCT/CN2016/078518 2015-04-21 2016-04-06 Composition de fibres de verre de haute performance, fibre de verre de cette dernière, et matériau composite WO2016169408A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
BR112017022438-0A BR112017022438B1 (pt) 2015-04-21 2016-04-06 Composição de fibra de vidro de alto desempenho, fibra de vidro da mesma e material compósito
US15/565,412 US10399889B2 (en) 2015-04-21 2016-04-06 High-performance glass fiber composition, glass fiber thereof, and composite material
ES16782556T ES2828726T3 (es) 2015-04-21 2016-04-06 Composición de fibra de vidrio de alto rendimiento, fibra de vidrio de la misma, y material compuesto
DK16782556.1T DK3287425T3 (da) 2015-04-21 2016-04-06 Højeffektiv glasfibersammensætning, glasfiber deraf og kompositmateriale
EP16782556.1A EP3287425B1 (fr) 2015-04-21 2016-04-06 Composition de fibres de verre de haute performance, fibre de verre de cette dernière, et matériau composite

Applications Claiming Priority (2)

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CN201510191134.0 2015-04-21
CN201510191134.0A CN105016622A (zh) 2015-04-21 2015-04-21 一种高性能玻璃纤维组合物及其玻璃纤维和复合材料

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WO2016169408A1 true WO2016169408A1 (fr) 2016-10-27

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US (1) US10399889B2 (fr)
EP (1) EP3287425B1 (fr)
CN (2) CN105016622A (fr)
BR (1) BR112017022438B1 (fr)
DK (1) DK3287425T3 (fr)
ES (1) ES2828726T3 (fr)
WO (1) WO2016169408A1 (fr)

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CN105819698B (zh) 2016-03-15 2018-09-14 巨石集团有限公司 一种高性能玻璃纤维组合物及其玻璃纤维和复合材料
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CN112811824A (zh) * 2021-03-12 2021-05-18 山东墨匠新材料科技有限公司 一种高耐碱性玻璃纤维组合物

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EP3287425A4 (fr) 2018-08-15
EP3287425B1 (fr) 2020-08-19
EP3287425A1 (fr) 2018-02-28
CN106938891A (zh) 2017-07-11
DK3287425T3 (da) 2020-09-14
BR112017022438B1 (pt) 2022-07-05
US10399889B2 (en) 2019-09-03
BR112017022438A2 (pt) 2018-07-10
ES2828726T3 (es) 2021-05-27
CN105016622A (zh) 2015-11-04
US20180118608A1 (en) 2018-05-03

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